HRID1795825

反应详情

EQUATION

反应方程式

HRID 1795825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Phenylboronic acid (417 mg), tetrakis(triphenylphosphine)palladium (132 mg), toluene (10 mL), 1,4-dioxane (5 mL), and a 2 mol/L aqueous solution of sodium carbonate (10 mL) were added to 5-[3,5-bis(trifluoromethyl)benzyl]-7-iodo-6-oxo-2,3,4,5-tetrahydro-6H-pyrido[2,3-b][1,5]oxazocine (1.00 g). While heated, the mixture was stirred for 7 hours under a stream of argon gas. The mixture was then diluted with ethyl acetate, was washed with a 2 mol/L aqueous solution of sodium carbonate, and was dried on anhydrous sodium sulfate. The solvent was removed and the resulting residue was recrystallized from isopropanol to obtain 5-[3,5-bis(trifluoromethyl)benzyl]-6-oxo-7-phenyl-2,3,4,5-tetrahydro-6H-pyrido[2,3-b][1,5]oxazocine (729 mg, 80%).

WORKUP

后处理

  1. temperatureWhile heated
  2. washwas washed with a 2 mol/L aqueous solution of sodium carbonate
  3. dry with materialwas dried on anhydrous sodium sulfate
  4. customThe solvent was removed
  5. customthe resulting residue was recrystallized from isopropanol